CN103132001B - Preparation of Y2O3Improved method for ceramic coating - Google Patents
Preparation of Y2O3Improved method for ceramic coating Download PDFInfo
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- CN103132001B CN103132001B CN201110394635.0A CN201110394635A CN103132001B CN 103132001 B CN103132001 B CN 103132001B CN 201110394635 A CN201110394635 A CN 201110394635A CN 103132001 B CN103132001 B CN 103132001B
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- plasma
- flow
- gas
- ceramic coating
- powder
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- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000005524 ceramic coating Methods 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 27
- 238000007750 plasma spraying Methods 0.000 claims abstract description 20
- 239000011248 coating agent Substances 0.000 claims abstract description 19
- 238000000576 coating method Methods 0.000 claims abstract description 19
- 230000008569 process Effects 0.000 claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000007789 gas Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000007921 spray Substances 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 238000007664 blowing Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000005488 sandblasting Methods 0.000 claims description 5
- 238000002203 pretreatment Methods 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000002826 coolant Substances 0.000 claims description 3
- 239000000112 cooling gas Substances 0.000 claims description 3
- 239000004576 sand Substances 0.000 claims description 2
- 238000005530 etching Methods 0.000 abstract description 12
- 238000005507 spraying Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000001020 plasma etching Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000010354 integration Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 238000004873 anchoring Methods 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229920002120 photoresistant polymer Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000009818 secondary granulation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000032258 transport Effects 0.000 description 1
Landscapes
- Coating By Spraying Or Casting (AREA)
Abstract
The invention relates to Y2O3The technical field of ceramic coating manufacturing, in particular to a method for preparing Y2O3An improved method of ceramic coating. Preparation Y2O3An improved method of ceramic coating comprising the steps of: step (1), selecting Y with purity of more than 99.95%2O3Powder; step (2), pretreating the surface of a base material to be sprayed; step (3), selecting Ar and H2The gas is ion gas, plasma spraying is carried out on the surface of the substrate by a plasma spraying device, and the plasma spraying is carried out on the surface of the substrateIntroducing O into the sub-flame flow2Preparation of Y2O3And (4) coating. The invention uses Ar/H2For spraying gas and adding O in plasma flame flow2To avoid Y2O3Is anoxic, Y prepared by the process of the invention2O3The coating is pure white, has uniform color, does not generate mottle, and has excellent etching resistance.
Description
Technical field
The present invention relates to Y
2o
3ceramic coating manufacturing technology field, is specifically related to one and prepares Y
2o
3improving one's methods of ceramic coating.
Background technology
At present, low-temperature plasma fine machining method is the gordian technique of material micro-nano processing, it is the basis of the technologies of preparing such as microelectronics, photoelectron, micromechanics, micro-optic, particularly in super large-scale integration manufacturing process, the operation of nearly 1/3rd is had to complete by means of plasma process, as plasma foil deposition, plasma etching and removing of photoresist by plasma etc.Wherein plasma etching is one of technical process of most critical, is the Micropicture realized in super large-scale integration production with high fidelity transfers to silicon chip irreplaceable technique from Lithographic template.
In etching process, owing to there is a large amount of living radicals with severe corrosive (as Cl
*, Cl
2 *, F
*, CF
*deng), the internal surface in their article on plasma etching technics chambeies also can produce corrosive nature, causes pollution, affects etching effect, and etching technics chamber can be made to lose efficacy.The plasma etching equipment of the early stage nineties, when smaller power and single plasma-generating source, aluminum substrate layer adds Al
2o
3coating just can meet the etch damage of plasma body to etching technics chamber.Enter into 300mm equipment, along with plasma power is increasing, the damage of plasma body to etching technics chamber wall is also increasing, makes, in the process of etching, following problem easily occurs: (1) particle; (2) process cavity wall disbonding, cause plasma body directly and aluminum substrate have an effect; (3) Al
2o
3the life-span of component is subject to more high-power restriction.So need to find a kind of new approach to carry out modification to etching technics inner cavity surface, meet the needs of etching technics.
Research shows, Y
2o
3coating has good provide protection to etching technics chamber.With Al
2o
3compare, Y
2o
3chemical property highly stable, there is excellent resistant to plasma etching performance, and and the reaction product YF that generates of CF system gas
3steam forces down, and is difficult to disperse as particle.With Y
2o
3powder, as spray material, utilizes air plasma spraying method, prepares the Y of single structure at etching technics inner cavity surface
2o
3coating, can effectively solve above-mentioned Al
2o
3the various problems that coating faces.
Air plasma spraying uses N
2, Ar, H
2and He etc. is as ion-gas, produce plasma high temperature and high speed jet through ionization, input material fusing or melting are ejected into the method that working-surface forms coating.Plasma arc extreme temperatures wherein, enough melts and comprises Y
2o
3at interior all high-melting-point ceramic powder; Melted powder kinetic energy in jet is large, with can fully launch after substrate contact, stacked, effectively improve anchoring strength of coating, reduce porosity.It is the gordian technique of preparation high-performance, high quality ceramic coating.
In plasma spray coating process, atmosphere surrounding can have the final performance of coating to be affected significantly.The selection principle of gas mainly considers practicality and economy.Plasma spraying is commonly used gas and is mainly contained N
2, Ar, H
2with He etc.N
2be diatomic gas, therefore the heat enthalpy value of plasma flame flow is higher, is conducive to the heating and melting of powder, have again higher ionization potential (15.8V), therefore the utilising efficiency of heat is high.Wide material sources simultaneously, therefore low price is the most frequently used working gas in plasma spraying.Its shortcoming is easy under high temperature and powdered reaction, and protected effect is poor.Ar is monoatomic gas, directly absorbs heat ionize in intensification ionization, and heat up very fast, do not react with any powder, protective value is good simultaneously.But its arc voltage is lower, and thermal conductivity is little, is seldom used alone, and expensive, originate less.He is also monoatomic gas, ionization voltage 24.5V, and heat enthalpy value is high, and viscosity is high, and a certain amount of He can effective stable arc.H
2ionization potential is low, has the highest thermal conductivity, contributes to powder smelting.Very strong reductibility is had to metallic substance, can anti-oxidation.In addition, in Ar, a small amount of H is counted
2, effectively can improve voltage and the power of plasma arcs.
If adopt Ar/He as ionized gas, spraying effect is desirable, and coating performance is better.In view of He is expensive, consider economic and practical, actual Y
2o
3plasma spray coating process adopts Ar/H
2as ionized gas to reduce costs, but so often Y can be caused
2o
3there is uneven black splotch in local in coating, thus affects coating performance.This is due to H
2with Y in spraying process
2o
3powder there occurs reduction reaction, makes the Y of anoxic condition
2o
3powder presents black.
Summary of the invention
One is the object of the present invention is to provide to prepare Y
2o
3improving one's methods of ceramic coating, eliminates variegated spot, improves the erosion resistance of coating.
In order to achieve the above object, the technical solution used in the present invention is:
One prepares Y
2o
3improving one's methods of ceramic coating, comprises the steps:
Step (1), selects the Y that purity is greater than 99.95%
2o
3powder;
Step (2), carries out pre-treatment to substrate surface to be sprayed;
Step (3), selects Ar and H
2gas is ionized gas, carries out plasma spraying by plasma-spraying device at described substrate surface, and in plasma flame flow, passes into O when described plasma spraying
2, prepare Y
2o
3coating.
In such scheme, the Y in described step (1)
2o
3the granularity of powder is 5 ~ 50 μm.
In such scheme, described step carries out pre-treatment to substrate surface to be sprayed in (2), specifically comprises the steps: to carry out sandblasting to substrate surface to be sprayed, and cleans with acetone.
In such scheme, the sand-blast material that described sandblasting adopts is white fused alumina, and sand size is 50 ~ 100 μm.
In such scheme, in described step (3), the flow of Ar gas is 40 ~ 90L/min, H
2the flow of gas is 5 ~ 20L/min.
In such scheme, in described step (3), the arc voltage of plasma-spraying device is 40 ~ 50V, and flame current is 800 ~ 900A, and powder feed rate is 15 ~ 100g/min, and spray distance is 80 ~ 135mm, and powder feeding angle is 50 ° ~ 90 °.
In such scheme, in the process of the middle plasma spraying of described step (3), air blowing method or recirculated water cooling method is adopted to cool described base material to be sprayed, in described air blowing method, the flow of cooling gas is 100 ~ 2000L/min, and in described recirculated water cooling method, the flow of water coolant is 10 ~ 500L/min.
In such scheme, described O
2carried in plasma flame flow by independent pipeline.
In such scheme, described O
2flow be 5-30L/min.
Compared with prior art, the beneficial effect that the technical solution used in the present invention produces is as follows:
The present invention is with Ar/H
2in plasma flame flow, O is added for spray gas
2, to avoid Y
2o
3anoxic, the Y prepared in the process of the present invention
2o
3coating is pure white, and variegated spot no longer appears in uniform color, and has excellent etch resistant performance.
Accompanying drawing explanation
Fig. 1 is the Y in the embodiment of the present invention
2o
3powder and O
2the schematic diagram of mode of movement.
Embodiment
Below in conjunction with drawings and Examples, technical solution of the present invention is described in detail.
As shown in Figure 1, the embodiment of the present invention provides one to prepare Y
2o
3improving one's methods of ceramic coating, specifically comprises the steps:
(1) Y is selected
2o
3powder, size range is 5 ~ 50 μm, and powder should have single Emission in Cubic structure; The initial size of powder is 40 ~ 60nm, and after secondary granulation, particle diameter is for being 5 ~ 50 μm, and the macrobead powder after granulation is the spherical of vesicular structure, is the hollow micron bead be assembled into by nanometer small-particle, has splendid mobility;
(2) carried out sandblasting to needs by the etching technics cavity wall of the aluminium base sprayed, sand-blast material is white fused alumina, and size range is 50 ~ 100 μm, and cleans with acetone;
(3) adopt Sluzer Metco 9MC plasma-spraying device 3 to carry out plasma spraying, spray gun type 9MB, by Y
2o
3powder and O
2use Y respectively
2o
3powdering inlet 1 and O
2entrance 2 transports, as shown in Figure 1, at Ar and H
2spray base material 4 under atmosphere surrounding, the flow of Ar gas is 40 ~ 90L/min, H
2the flow of gas is 5 ~ 20L/min, and the arc voltage of plasma-spraying device is 40 ~ 50V, and flame current is 800 ~ 900A, and powder feed rate is 15 ~ 100g/min, powder feeding angle 50 ° ~ 90 °, and spray distance is 80 ~ 135mm; In spraying process, adopt air blowing method or recirculated water cooling method to cool matrix, when adopting air blowing method, the flow of cooling gas is 100 ~ 2000L/min, and when adopting recirculated water cooling method, the flow of water coolant is 10 ~ 500L/min; O
2flow also very large on the impact of coating quality, flow control is at 5-30L/min, if the too small meeting of flow makes powder be difficult to through O
2fully oxidized, excessive, powder can be made to depart from jet-core region, and cause coating to be loosened, bonding strength reduces; Through above-mentioned steps, finally prepare Y
2o
3ceramic coating.
The present invention is with Ar/H
2in plasma flame flow, O is added for spray gas
2, to avoid Y
2o
3anoxic, the Y prepared in the process of the present invention
2o
3coating is pure white, and variegated spot no longer appears in uniform color, and has excellent etch resistant performance.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. prepare Y for one kind
2o
3improving one's methods of ceramic coating, is characterized in that, comprises the steps:
Step (1), selects the Y that purity is greater than 99.95%
2o
3powder;
Step (2), carries out pre-treatment to substrate surface to be sprayed;
Step (3), selects Ar and H
2gas is ionized gas, carries out plasma spraying by plasma-spraying device at described substrate surface, and in plasma flame flow, passes into O when described plasma spraying
2, prepare Y
2o
3coating;
Wherein, in described step (3), the flow of Ar gas is 40 ~ 90L/min, H
2the flow of gas is 5 ~ 20L/min;
In the process of the middle plasma spraying of described step (3), air blowing method or recirculated water cooling method is adopted to cool described base material to be sprayed, in described air blowing method, the flow of cooling gas is 100 ~ 2000L/min, and in described recirculated water cooling method, the flow of water coolant is 10 ~ 500L/min;
Wherein, the Y in described step (1)
2o
3the granularity of powder is 5 ~ 50 μm;
Wherein, described step carries out pre-treatment to substrate surface to be sprayed in (2), specifically comprises the steps: to carry out sandblasting to substrate surface to be sprayed, and cleans with acetone.
2. prepare Y as claimed in claim 1
2o
3improving one's methods of ceramic coating, is characterized in that, the sand-blast material that described sandblasting adopts is white fused alumina, and sand size is 50 ~ 100 μm.
3. prepare Y as claimed in claim 1
2o
3improving one's methods of ceramic coating, is characterized in that, in described step (3), the arc voltage of plasma-spraying device is 40 ~ 50V, flame current is 800 ~ 900A, powder feed rate is 15 ~ 100g/min, and spray distance is 80 ~ 135mm, and powder feeding angle is 50 ° ~ 90 °.
4. prepare Y as claimed in claim 1
2o
3improving one's methods of ceramic coating, is characterized in that, described O
2carried in plasma flame flow by independent pipeline.
5. prepare Y as claimed in claim 1
2o
3improving one's methods of ceramic coating, is characterized in that, described O
2flow be 5-30L/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110394635.0A CN103132001B (en) | 2011-12-02 | 2011-12-02 | Preparation of Y2O3Improved method for ceramic coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110394635.0A CN103132001B (en) | 2011-12-02 | 2011-12-02 | Preparation of Y2O3Improved method for ceramic coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103132001A CN103132001A (en) | 2013-06-05 |
| CN103132001B true CN103132001B (en) | 2015-07-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110394635.0A Active CN103132001B (en) | 2011-12-02 | 2011-12-02 | Preparation of Y2O3Improved method for ceramic coating |
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|---|---|
| CN (1) | CN103132001B (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5623619B1 (en) * | 2013-12-02 | 2014-11-12 | 倉敷ボーリング機工株式会社 | Manufacturing method of chamber member for dry etching |
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|---|---|---|---|---|
| CN1687486A (en) * | 2005-02-17 | 2005-10-26 | 建设工业(集团)有限责任公司 | Method for plating hard chromium on surface of metallic material |
| US7494723B2 (en) * | 2005-07-29 | 2009-02-24 | Tocalo Co., Ltd. | Y2O3 spray-coated member and production method thereof |
| JP4981291B2 (en) * | 2005-09-30 | 2012-07-18 | 株式会社フジミインコーポレーテッド | Thermal spray powder and method of forming thermal spray coating |
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| Publication number | Publication date |
|---|---|
| CN103132001A (en) | 2013-06-05 |
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